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Tert-butyl acrylamide sulfonic acid production method

A technology of tert-butylacrylamide sulfonic acid and a production method, which is applied in the production field of organic compounds, can solve problems such as increasing production costs, and achieve the effect of improving economic benefits

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two methods not only do not produce economic benefits, but also increase production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This embodiment is used to illustrate the production method of ATBS provided by the present invention.

[0042] (1) Add 496g of acrylonitrile containing 0.25% by mass of water into the mixer, lower the temperature to -5°C, and then add 73.6g of SO 3 Fuming sulfuric acid with a content of 3% enters steady state operation after stirring evenly. The specific method is: add acrylonitrile with 0.25% water content to the above-mentioned mixer through a flow meter at a flow rate of 248.0g / h by a metering pump, and add oleum at the same time, wherein free SO 3 The mass content is 3%, and the metering pump is added through a meter at a flow rate of 36.8g / h to obtain a mixed solution.

[0043] (2) The mixed liquid flows continuously into the horizontal reactor through the overflow port in the middle of the mixer. The horizontal reactor has three isobutene inlet pipelines. After the isobutene is vaporized, it is continuously fed into the horizontal reactor at a total flow rate of...

Embodiment 2

[0047] Steps 1)-3) are the same as in Example 1. In step 4), chloroform is used as the processing solvent, and the filter cake is vacuum-dried. The drying temperature is 100°C, and the drying pressure is 10KPa (gauge pressure) to obtain a dried filter cake. A total of 130.2g, the main component is ATBS, and the purity is 98.3% (mass) by liquid chromatography; the filtrate is distilled under reduced pressure, and the solvent is condensed for reuse. The main component of the solid obtained after distillation is tert-butylacrylamide, a total of 19.4 g, the purity was 95.0% (mass) by liquid chromatography.

Embodiment 3

[0049] Steps 1)-3) are the same as in Example 1, the stirring time in step 4) is fixed at 300min, and the filter cake is vacuum-dried. The drying temperature is 100°C, and the drying pressure is 10KPa (gauge pressure). The cake was 130.4g in total, the main component was ATBS, and the purity was 97.2% (mass) by liquid chromatography; the filtrate was distilled under reduced pressure, and the solvent was condensed and reused. The main component of the solid obtained after distillation was tert-butylacrylamide. 19.4g, the purity by liquid chromatography analysis is 96.2% (mass).

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Abstract

The present invention relates to a tert-butyl acrylamide sulfonic acid production method, which comprises: 1) forming an acrylonitrile solution containing a sulfonating agent; 2) continuously introducing the solution into a horizontal stirring reactor to contact isobutene so as to form a slurry product; 3) filtering the slurry product to obtain the filter cake containing tert-butyl acrylamide sulfonic acid and the filtrate; 4) drying the filter cake obtained in the step 3) to obtain a tert-butyl acrylamide sulfonic acid crude product; 5) adopting an acetic acid aqueous solution to carry out recrystallization purification on the tert-butyl acrylamide sulfonic acid crude product obtained in the step 4) to obtain the tert-butyl acrylamide sulfonic acid with the mass content of more than 99.3% and the remaining waste liquid; and 6) evaporating the filtrate in the step 3) and / or the remaining waste liquid in the step 4) to obtain the waste residue, carrying out mixing contact on the waste residue and a treatment solvent, and carrying out solid-liquid separation to obtain the tert-butyl acrylamide sulfonic acid and the tert-butyl acrylamide.

Description

technical field [0001] The invention relates to a production method of an organic compound, in particular to a production method of tert-butylacrylamide sulfonic acid. Background technique [0002] Tert-butylacrylamide sulfonic acid (molecular formula C 7 h 13 NO 4 S, hereinafter referred to as ATBS) is a multifunctional water-soluble anionic monomer, which is easy to polymerize due to its molecular structure with carbon-carbon double bonds and salt-insensitive sulfonic acid groups, and its homopolymerization and copolymers have many special properties. It has broad application prospects and can be widely used in oilfield chemistry, water treatment agents, chemical fibers, plastics, printing and dyeing, coatings, surfactants, antistatic agents, ceramics, photography, washing aids, ion exchange resins, and gas separation membranes. , electronics industry and other fields. [0003] At present, the most typical process for producing ATBS is to prepare ATBS by reacting acryl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/15C07C303/02
Inventor 李斗星齐兰芝黄凤兴穆晓蕾贾春革
Owner CHINA PETROLEUM & CHEM CORP
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